HRID2268416

反应详情

EQUATION

反应方程式

HRID 2268416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

{9-[(2R,3R,4R,5R)-3,4-bis{[tert-butyl(dimethyl)silyl]oxy}-5-(methoxymethyl)tetrahydro-2-furanyl]-6-[(2,2-diphenylethyl)amino]-9H-purin-2-yl}methyl methanesulfonate (240 mg, 0.3 mmol) (preparation 16) was dissolved in stirred tetrahydrofuran (1 ml) and a 1 molar solution of tetra-n-butylammonium fluoride in tetrahydrofuran (0.6 ml, 0.6 mmol) added. The reaction mixture was stirred at room temperature for 24 hr. The solvent was removed under reduced pressure and the residue purified by column chromatography on silica gel eluting with a gradient system of dichloromethane:methanol (95:5) increasing in polarity to dichloromethane:methanol (90:10). This gave the title compound (140 mg) as a foam. MS: 570 (MH+).

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customthe residue purified by column chromatography on silica gel eluting with a gradient system of dichloromethane:methanol (95:5)
  3. temperatureincreasing in polarity to dichloromethane:methanol (90:10)